Method and equipment for synthesizing and preparing creatine monohydrate

Abstract

The invention relates to the technical field of creatine monohydrate preparation, and discloses a creatine monohydrate synthesis preparation method and equipment, and the method comprises the following steps: S1, adding chloroacetic acid and methylamine water into a reaction kettle, and carrying out a reaction at 20-30 DEG C for 8-10 h; s2, the temperature is raised to 80-95 DEG C, the heating time is 1-3 h, and unreacted methylamine is recovered; s3, adding a sodium hydroxide solution into the solution obtained in S2, and neutralizing reaction by-products; s4, heating to 105-110 DEG C, and concentrating under reduced pressure to obtain a sarcosine aqueous solution; s5, filtering the sarcosine aqueous solution in the step S4, and taking filtrate into a crystallizer; s6, continuously introducing ammonia gas into the crystallizer, stirring, adjusting the pH value of the solution to 9-12, and then performing crystallization treatment on the reaction solution to obtain creatine crystals; and S7, filtering, washing and drying the creatine crystals in the step S6 to obtain crude creatine monohydrate. The method has the following advantages and effects that the reaction efficiency and the conversion rate are relatively high, the produced creatine monohydrate is high in purity and stable in quality, and the requirements of different fields on the product quality can be met.

Description

Technical Field

[0001] The present invention relates to the technical field of monohydrate creatine preparation, and particularly relates to a method and equipment for synthesizing and preparing monohydrate creatine. Background Art

[0002] Monohydrate creatine can inhibit the generation of muscle fatigue factors, relieve fatigue and tension, restore physical strength, accelerate the synthesis of human proteins, make muscles stronger, enhance muscle elasticity, reduce cholesterol, blood lipid and blood sugar levels, improve muscle atrophy in the elderly, and delay aging. Monohydrate creatine is known as one of the most popular and effective nutritional supplements, and its status is high enough to keep pace with protein products.

[0003] In the prior art, for example, a method for preparing high-purity monohydrate creatine disclosed in a Chinese patent with the patent publication number CN115636772B. The preparation method of the present invention uses sodium sarcosinate and monocyanamide as raw materials. By controlling the reaction conditions, a wet crude product of monohydrate creatine is first prepared, and then the wet crude product of monohydrate creatine is dissolved by heating with pure water, and then the cooling crystallization is controlled. After that, it is separated and dried to obtain a high-purity monohydrate creatine product. The mother liquor can be concentrated, purified, cooled and crystallized to continue to recover monohydrate creatine. The monohydrate creatine product obtained by the present invention has high purity, high yield, and a simple and feasible treatment process.

[0004] However, in the production of existing monohydrate creatine, it is necessary to crystallize the raw materials through a crystallizer. When the monohydrate creatine raw materials form crystal particles, the discharge of the crystal particles is not convenient enough, and the crystal particles are doped with dust inside. The crystal particles and the dust cannot be separated and need to be separated separately, which further increases the production steps. Therefore, the above problems need to be improved. Summary of the Invention

[0005] A method for synthesizing and preparing monohydrate creatine, characterized by comprising the following steps: S1. Put chloroacetic acid and aqueous methylamine into a reaction kettle and react at 20°C - 30°C for 8 - 10 h; S2. Raise the temperature of the reaction kettle to 80°C - 95°C, heat for 1 - 3 h, and recover the unreacted methylamine; S3. Put a sodium hydroxide solution into S2 to neutralize the reaction by-products; S4. Raise the temperature to 105°C - 110°C, and concentrate under reduced pressure to obtain an aqueous sarcosine solution; S5. Filter the aqueous sarcosine solution in S4, and take the filtrate into a crystallizer; S6. Continuously introduce ammonia gas into the crystallizer and stir, adjust the pH of the solution to 9 - 12, and then perform crystallization treatment on the reaction solution to obtain creatine crystals; S7. Filter, wash, and dry the creatine crystals in S6 to obtain crude monohydrate creatine.

[0006] By adopting the above technical solutions, the types of reactants in the above process are few, the production process is controllable, and it has high reaction efficiency and conversion rate. The monohydrate creatine produced has high purity and stable quality, and can meet the requirements of different fields for product quality.

[0007] The crystallizer includes a body, inside which a crystallization chamber is fixedly connected. At the bottom of the crystallization chamber, a discharge pipe is fixedly connected. An electric gate is arranged at the port of the discharge pipe. Inside the body, a first motor is fixedly connected. The output end of the first motor is fixedly connected with a drive shaft, which extends into the interior of the discharge pipe. A spiral blade is fixedly connected to the outside of the drive shaft. A feed bin is fixedly connected to the outside of the body. Inside the feed bin, a blanking hopper is fixedly connected. A feed plate is fixedly connected to the inside of the feed bin. A blanking hole is formed in the feed plate. A cylinder is fixedly installed on the outside of the feed bin. The output end of the cylinder is fixedly connected with a push plate, and a storage box is arranged below the push plate.

[0008] By adopting the above technical solution, after the raw materials inside the crystallization chamber form crystals, the port of the discharge pipe is opened through the electric gate, so that the crystal particles enter the interior of the discharge pipe. The first motor is started, and the first motor drives the spiral blade to rotate through the drive shaft. The spiral blade is spiral, so that the crystal particles are conveyed through the spiral blade. The discharge pipe is arranged above the feed bin, and the crystal particles inside the discharge pipe will be conveyed into the interior of the feed bin. The blanking hopper is trapezoidal, which can prevent the material from overflowing to the outside of the feed bin. The crystal particles will fall into the feed plate inside the feed bin. The cylinder is started, so that the cylinder drives the push plate to expand and contract. During the expansion and contraction process, the push plate will contact the crystal particles. During this process, the crystal particles will be pushed to the outside of the feed bin by the push plate, and the dust inside the crystal particles will fall into the interior of the storage box through the blanking hole, so that the crystal particles can complete dust separation during the discharging process, greatly improving the production efficiency of the crystal particles.

[0009] A further setting of the present invention is that the number of the blanking holes is several, and several of the blanking holes are distributed in the form of a rectangular array.

[0010] By adopting the above technical solution, through the arrangement of multiple blanking holes, the dust enters the interior of the storage box through the multiple blanking holes.

[0011] A further setting of the present invention is that a frame is fixedly connected to the inside of the feed bin, and a horizontal shaft is rotatably connected to the inside of the frame.

[0012] By adopting the above technical solution, the storage box is lapped on the top of the horizontal shaft. When it is necessary to process the dust inside the storage box, the storage box is moved so that the storage box slides on the outside of the horizontal shaft, and then the storage box can be taken out of the feed bin.

[0013] A further setting of the present invention is that the number of the horizontal shafts is several, and the distances between every two of the several horizontal shafts are equal.

[0014] By adopting the above technical solution, multiple horizontal shafts are rotatably connected inside the frame, the storage box is in contact with the multiple horizontal shafts, and the storage box is supported by the multiple horizontal shafts.

[0015] A further setting of the present invention is that a heating mechanism is arranged inside the crystallization chamber, and a condensation mechanism is fixedly connected inside the machine body.

[0016] By adopting the above technical solution, the heating mechanism heats the raw materials inside the crystallization chamber, and the condensation mechanism cools the crystallization chamber. The alternating of heat and cold causes the raw materials to form crystals.

[0017] A further setting of the present invention is that a raw material box is fixedly connected to the inner bottom wall of the machine body, a pump body is arranged inside the raw material box, and the output end of the pump body is fixedly connected to a feeding pipe.

[0018] By adopting the above technical solution, the raw material box stores the raw materials. Starting the pump body causes the pump body to pump the raw materials inside the raw material box into the feeding pipe. The feeding pipe is fixed at the bottom of the crystallization chamber, so that the raw materials enter the inside of the crystallization chamber.

[0019] A further setting of the present invention is that a second motor is fixedly installed outside the machine body, and the output end of the second motor is fixedly connected to a stirring shaft.

[0020] By adopting the above technical solution, starting the second motor causes the second motor to drive the stirring shaft to rotate.

[0021] A further setting of the present invention is that stirring blades are fixedly connected to the outside of the stirring shaft, and the number of the stirring blades is several.

[0022] By adopting the above technical solution, multiple stirring blades are distributed on the outside of the stirring shaft. The raw materials inside the crystallization chamber are stirred by the multiple stirring blades, so as to improve the uniformity of heat reception of the raw materials.

[0023] A further setting of the present invention is that bases are fixedly connected to the bottoms of the machine body and the storage bin, and moisture-proof pads are fixedly connected to the bottoms of the bases.

[0024] By adopting the above technical solution, the bases and the moisture-proof pads support the machine body and the storage bin.

[0025] A further setting of the present invention is that motor boxes are arranged outside both the first motor and the second motor.

[0026] By adopting the above technical solution, the number of the motor boxes is two, and the two motor boxes are respectively and fixedly arranged inside and outside the machine body, and the two motor boxes respectively wrap the first motor and the second motor, so as to protect the first motor and the second motor.

[0027] The beneficial effects of the present invention are as follows:

[0028] 1. Through the settings among the machine body, crystallization chamber, discharge pipe, electric gate, first motor, drive shaft, spiral blade, storage bin, feed hopper, feed plate, feed hole, cylinder, push plate and storage box, after the raw materials inside the crystallization chamber form crystals, the port of the discharge pipe is opened through the electric gate, so that the crystal particles enter the inside of the discharge pipe. Start the first motor, so that the first motor drives the spiral blade to rotate through the drive shaft. The spiral blade is spiral, and then the crystal particles are conveyed through the spiral blade. The discharge pipe is arranged above the storage bin, and the crystal particles inside the discharge pipe will be conveyed into the storage bin. The feed hopper is trapezoidal, which can prevent the materials from overflowing outside the storage bin. The crystal particles will fall into the feed plate inside the storage bin. Start the cylinder, so that the cylinder drives the push plate to expand and contract. During the expansion and contraction process, the push plate will contact the crystal particles. During this process, the crystal particles will be pushed outside the storage bin by the push plate, and the dust inside the crystal particles will fall into the storage box through the feed hole, so that the crystal particles can complete dust separation during the discharging process, greatly improving the production efficiency of the crystal particles.

[0029] 2. Through the settings among the frame, horizontal axis, heating mechanism, condensation mechanism, raw material box, feeding pipe, second motor, stirring shaft and stirring blades, the storage box is lapped on the top of the horizontal axis. When it is necessary to process the dust inside the storage box, move the storage box so that the storage box slides outside the horizontal axis, and then the storage box can be taken out of the storage bin. The raw material box stores the raw materials. Start the pump body, so that the pump body pumps the raw materials inside the raw material box into the feeding pipe. The feeding pipe is fixed at the bottom of the crystallization chamber, so that the raw materials enter the inside of the crystallization chamber. Start the second motor, so that the second motor drives the stirring shaft to rotate. A plurality of stirring blades are distributed outside the stirring shaft, and the raw materials inside the crystallization chamber are stirred through the plurality of stirring blades, which can improve the uniformity of heat reception of the raw materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following will briefly introduce the drawings required for the description of the embodiments. Obviously, the following drawings are only some embodiments of the present invention. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative efforts.

[0031] Figure 1 It is a schematic structural diagram of the present invention;

[0032] Figure 2 It is a schematic diagram of the internal structure of the machine body of the present invention;

[0033] Figure 3Schematic diagram of the internal structure of the discharge pipe of the present invention;

[0034] Figure 4 Schematic diagram of the internal structure of the storage bin of the present invention;

[0035] Figure 5 For the present invention Figure 4 Enlarged schematic diagram of part A in the present invention.

[0036] In the figure, 1, body; 2, crystallization chamber; 3, discharge pipe; 4, electric gate; 5, first motor; 6, drive shaft; 7, spiral blade; 8, storage bin; 9, hopper; 10, material plate; 11, discharge hole; 12, cylinder; 13, push plate; 14, storage box; 15, frame; 16, horizontal shaft; 17, heating mechanism; 18, condensation mechanism; 19, raw material box; 20, feeding pipe; 21, second motor; 22, stirring shaft; 23, stirring blade; 24, base; 25, motor box. Detailed implementation manners

[0037] The technical solutions of the present invention will be clearly and completely described below in conjunction with specific embodiments. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0038] A crystallization device for producing creatine monohydrate, as Figures 1-5As shown in the figure, it includes a machine body 1. Inside the machine body 1, a crystallization chamber 2 is fixedly connected. At the bottom of the crystallization chamber 2, a discharge pipe 3 is fixedly connected. At the port of the discharge pipe 3, an electric gate 4 is provided. Inside the machine body 1, a first motor 5 is fixedly connected. The output end of the first motor 5 is fixedly connected with a drive shaft 6. The drive shaft 6 extends into the interior of the discharge pipe 3. Outside the drive shaft 6, a spiral blade 7 is fixedly connected. Outside the machine body 1, a feed bin 8 is fixedly connected. Inside the feed bin 8, a feeding hopper 9 is fixedly connected. Inside the feed bin 8, a feed plate 10 is fixedly connected. Inside the feed plate 10, a feeding hole 11 is formed. Outside the feed bin 8, a cylinder 12 is fixedly installed. The output end of the cylinder 12 is fixedly connected with a push plate 13. Below the push plate 13, a storage box 14 is provided. After the raw materials inside the crystallization chamber 2 form crystals, the port of the discharge pipe 3 is opened through the electric gate 4, so that the crystal particles enter the interior of the discharge pipe 3. The first motor 5 is started, so that the first motor 5 drives the spiral blade 7 to rotate through the drive shaft 6. The spiral blade 7 is spiral, so that the crystal particles are conveyed through the spiral blade 7. The discharge pipe 3 is arranged above the feed bin 8. The crystal particles inside the discharge pipe 3 will be conveyed into the interior of the feed bin 8. The feeding hopper 9 is trapezoidal, so as to prevent the materials from overflowing outside the feed bin 8. The crystal particles will fall into the feed plate 10 inside the feed bin 8. The cylinder 12 is started, so that the cylinder 12 drives the push plate 13 to expand and contract. During the expansion and contraction process, the push plate 13 will contact the crystal particles. During this process, the crystal particles will be pushed outside the feed bin 8 by the push plate 13. The dust inside the crystal particles will fall into the interior of the storage box 14 through the feeding holes 11, so that the crystal particles can complete dust separation during the discharging process, greatly improving the production efficiency of the crystal particles. The number of the feeding holes 11 is several, and several feeding holes 11 are distributed in the form of a rectangular array. Through the arrangement of multiple feeding holes 11, the dust enters the interior of the storage box 14 through the multiple feeding holes 11. Inside the feed bin 8, a frame 15 is fixedly connected. Inside the frame 15, a transverse shaft 16 is rotatably connected. The storage box 14 is lapped on the top of the transverse shaft 16. When it is necessary to process the dust inside the storage box 14, the storage box 14 is moved so that the storage box 14 slides outside the transverse shaft 16, so that the storage box 14 can be taken out inside the feed bin 8. The number of the transverse shafts 16 is several, and the distance between every two of the several transverse shafts 16 is equal. The multiple transverse shafts 16 are all rotatably connected inside the frame 15. The storage box 14 contacts the multiple transverse shafts 16, and the storage box 14 is supported by the multiple transverse shafts 16. Inside the crystallization chamber 2, a heating mechanism 17 is provided. Inside the machine body 1, a condensation mechanism 18 is fixedly connected. The heating mechanism 17 heats the raw materials inside the crystallization chamber 2, and the condensation mechanism 18 cools the crystallization chamber 2. The alternating of heat and cold makes the raw materials form crystals. On the inner bottom wall of the machine body 1, a raw material box 19 is fixedly connected. Inside the raw material box 19, a pump body is provided. The output end of the pump body is fixedly connected with a feeding pipe 20. The raw material box 19 stores the raw materials.Start the pump body so that the pump body pumps the raw materials inside the raw material tank 19 into the inside of the feeding pipe 20. The feeding pipe 20 is fixed to the bottom of the crystallization chamber 2, so that the raw materials enter the inside of the crystallization chamber 2. A second motor 21 is fixedly installed outside the machine body 1. The output end of the second motor 21 is fixedly connected to a stirring shaft 22. Start the second motor 21 so that the second motor 21 drives the stirring shaft 22 to rotate. A stirring blade 23 is fixedly connected to the outside of the stirring shaft 22. The number of stirring blades 23 is several. A plurality of stirring blades 23 are distributed outside the stirring shaft 22. Stir the raw materials inside the crystallization chamber 2 through the plurality of stirring blades 23, so as to improve the uniformity of heat absorption of the raw materials. The bottoms of the machine body 1 and the material bin 8 are both fixedly connected to a base 24. The bottom of the base 24 is fixedly connected to a moisture-proof pad. The base 24 and the moisture-proof pad support the machine body 1 and the material bin 8. Motor boxes 25 are arranged outside the first motor 5 and the second motor 21. The number of motor boxes 25 is two, and the two motor boxes 25 are fixedly distributed inside and outside the machine body 1, and the two motor boxes 25 respectively wrap the first motor 5 and the second motor 21, so as to protect the first motor 5 and the second motor 21.,

[0039] Further, after the raw materials inside the crystallization chamber 2 form crystals, the port of the discharge pipe 3 is opened through the electric gate 4, so that the crystal grains enter the inside of the discharge pipe 3. The first motor 5 is started, and the first motor 5 drives the spiral blade 7 to rotate through the drive shaft 6. The spiral blade 7 is spiral, so that the crystal grains are conveyed through the spiral blade 7. The discharge pipe 3 is arranged above the storage bin 8, and the crystal grains inside the discharge pipe 3 will be conveyed into the storage bin 8. The feeding hopper 9 is trapezoidal, so as to prevent the materials from overflowing outside the storage bin 8. The crystal grains will fall into the material plate 10 inside the storage bin 8. The air cylinder 12 is started, and the air cylinder 12 drives the push plate 13 to expand and contract. During the expansion and contraction process, the push plate 13 will contact the crystal grains. During this process, the crystal grains will be pushed outside the storage bin 8 by the push plate 13. The dust inside the crystal grains will fall into the storage box 14 through the material discharge hole 11, so that the crystal grains can complete dust separation during the discharging process, greatly improving the production efficiency of the crystal grains. The storage box 14 is lapped on the top of the cross shaft 16. When it is necessary to process the dust inside the storage box 14, the storage box 14 is moved so that the storage box 14 slides outside the cross shaft 16, so that the storage box 14 can be taken out of the storage bin 8. The raw material box 19 stores the raw materials. The pump body is started, and the pump body pumps the raw materials inside the raw material box 19 into the inside of the feeding pipe 20. The feeding pipe 20 is fixed at the bottom of the crystallization chamber 2, so that the raw materials enter the inside of the crystallization chamber 2. The second motor 21 is started, and the second motor 21 drives the stirring shaft 22 to rotate. A plurality of stirring blades 23 are distributed on the outside of the stirring shaft 22, and the raw materials inside the crystallization chamber 2 are stirred through the plurality of stirring blades 23, so as to improve the heat uniformity of the raw materials.

[0040] A preparation method of creatine monohydrate synthesis comprises the following steps

[0041] S1. Put chloroacetic acid and aqueous methylamine into a reaction kettle and react at 20°C - 30°C for 8 - 10 h;

[0042] S2. Heat the reaction kettle to 80°C - 95°C, with a heating time of 1 - 3 h, and recover the unreacted methylamine;

[0043] S3. Put sodium hydroxide solution into S2 to neutralize the reaction by-products;

[0044] S4. Heat to 105°C - 110°C and concentrate under reduced pressure to obtain an aqueous solution of sarcosine;

[0045] S5. Filter the aqueous solution of sarcosine in S4 and take the filtrate into a crystallizer;

[0046] S6. Continuously introduce ammonia gas into the crystallizer and stir, adjust the pH of the solution to 9 - 12, and then perform crystallization treatment on the reaction solution to obtain creatine crystals;

[0047] S7. Filter, wash, and dry the creatine crystals in S6 to obtain crude creatine monohydrate.

Claims

1. A method for synthesizing creatine monohydrate, characterized in that: The following steps are included S1. Add chloroacetic acid and methylamine water into a reaction kettle and react at 20°C-30°C for 8-10h; S2, heating the reactor to 80°C-95°C for 1-3h, and recovering unreacted methylamine; S3, adding sodium hydroxide solution into S2 to neutralize the reaction by-products; S4, heating to 105°C-110°C, concentrating under reduced pressure to obtain a sarcosine aqueous solution; S5, filtering the sarcosine aqueous solution in S4, and taking the filtrate into a crystallizer; S6, continuously introducing ammonia gas into the crystallizer with stirring, adjusting the pH value of the solution to 9-12, and then performing crystallization treatment on the reaction solution to obtain creatine crystals; S7. Filter, wash and dry the creatine crystals in S6 to obtain crude creatine monohydrate.

2. A creatine monohydrate preparation device according to claim 1, characterized in that: The crystallizer comprises a body (1), characterized in that: a crystallization chamber (2) is fixedly connected to the inside of the body (1), a discharge pipe (3) is fixedly connected to the bottom of the crystallization chamber (2), an electric gate (4) is arranged at the end of the discharge pipe (3), a first motor (5) is fixedly connected to the inside of the body (1), a drive shaft (6) is fixedly connected to the output end of the first motor (5), the drive shaft (6) extends to the inside of the discharge pipe (3), and the outside of the drive shaft (6) is A spiral blade (7) is fixedly connected, a silo (8) is fixedly connected to the outside of the body (1), a lower hopper (9) is fixedly connected to the inside of the silo (8), a material plate (10) is fixedly connected to the inside of the silo (8), a material discharge hole (11) is provided inside the material plate (10), a cylinder (12) is fixedly installed on the outside of the silo (8), a push plate (13) is fixedly connected to the output end of the cylinder (12), and a material storage box (14) is provided below the push plate (13).

3. A creatine monohydrate preparation device according to claim 2, characterized in that: The number of the material discharge holes (11) is several, and the several material discharge holes (11) are distributed in the form of a rectangular array.

4. A creatine monohydrate preparation device according to claim 3, characterized in that: The interior of the silo (8) is fixedly connected to a frame (15), and the interior of the frame (15) is rotatably connected to a transverse axis (16). There are a plurality of transverse axes (16), and the spacing between any two of the transverse axes (16) is equal.

5. A creatine monohydrate preparation device according to claim 4, characterized in that: A heating mechanism (17) is provided inside the crystallization chamber (2), and a condensing mechanism (18) is fixedly connected inside the machine body (1).

6. A creatine monohydrate preparation device according to claim 5, characterized in that: The inner bottom wall of the machine body (1) is fixedly connected to a raw material box (19), a pump body is arranged inside the raw material box (19), and a feed pipe (20) is fixedly connected to the output end of the pump body.

7. A creatine monohydrate preparation device according to claim 6, characterized in that: A second motor (21) is fixedly mounted on the outside of the machine body (1), and a stirring shaft (22) is fixedly connected to the output end of the second motor (21).

8. The creatine monohydrate preparation device according to claim 7, characterized in that: The outside of the stirring shaft (22) is fixedly connected with a stirring blade (23), and the number of the stirring blades (23) is several.

9. A creatine monohydrate preparation device according to claim 8, characterized in that: The bottoms of the machine body (1) and the silo (8) are both fixedly connected to a base (24), and the bottom of the base (24) is fixedly connected to a moisture-proof pad.

10. The creatine monohydrate preparation device according to claim 9, characterized in that: A motor box (25) is disposed outside the first motor (5) and the second motor (21).

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